US4507189A - Process of physical vapor deposition - Google Patents
Process of physical vapor deposition Download PDFInfo
- Publication number
- US4507189A US4507189A US06/316,906 US31690681A US4507189A US 4507189 A US4507189 A US 4507189A US 31690681 A US31690681 A US 31690681A US 4507189 A US4507189 A US 4507189A
- Authority
- US
- United States
- Prior art keywords
- vapor deposition
- physical vapor
- hydrogen
- tools
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
- B23P15/28—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass cutting tools
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
- C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
Definitions
- the present invention relates to a process of physical vapor deposition which homogeneously and tightly coats hard compounds on the surface of cutting tools, parts requiring wear resistance or ornaments such as a watch case and the like in order to improve wear resistance, heat resistance, corrosion resistance, appearance and the like of said tools, parts or ornaments.
- Said hard compounds generally include carbides, nitrides and oxides of metals, which have higher hardness and chemical stability, belonging to IVb group (titanium, zirconium, hafnium), Vb group (vanadium, niobium, tantalum), VIb group (chromium, molybdenum, tungsten) and the like; or aluminium oxide or zirconium oxide; or solid solution of these compounds.
- the coating may be used in the form of a single layer or multiple layers.
- the present invention relates to a method of coating said compounds homogeneously and tightly.
- the present invention is not limited to specific types and compositions of said hard compounds.
- Various kinds of coating methods including chemical vapor deposition processes, physical vapor deposition processes and spray coating methods, have been used. Above all, the physical vapor deposition process has been applied in increasingly wide fields recently because said hard compounds can be tightly coated even at lower temperatures of room temperature to 500° C. and as a result the properties and precision of the substrates, that is to say said tools and parts, are not damaged.
- Argon is used because it is inert and as a result it does not react chemically with said substrates, the sputtering yield of argon being large due to the larger molecular weight thereof. Also it is comparatively inexpensive and easily obtainable. Moreover nitrogen may be used for similar reasons.
- the surface of said substrates is cleaned only by the sputtering action in said sputter cleaning using argon or nitrogen and as a result, the surface of convex portions, pointed end portions and corner portions of said substrates, with which said positive ions of gas collide with larger energy, can be easily cleaned while the surface of concave portions and the central portion of said substrates, with which said positive ions of gas collide with smaller energy, are difficultly cleaned.
- the surface of concave portions and the central portion of said substrates are contaminated by the accumulation of oxides and the like coming from said convex portions, pointed portions and corner portions of said substrates which can be easily sputtered.
- the known method of sputter cleaning has never given a coating of homogeneous adhesive strength.
- FIG. 1 depicts an example of apparatus used in the present invention.
- FIG. 2 is a perspective view showing an example of tips used in the preferred embodiments of the present invention.
- FIG. 3 depicts a holder provided with a tip mounted thereon.
- FIG. 4 is a perspective view showing the state in which a tip is mounted on a holder.
- FIG. 5 shows the positions A to I at which a tip is tested on indentations.
- the present invention is characterized by using hydrogen or a gaseous mixture of hydrogen and inert gas as the atmosphere in order to solve the problem of heterogeneously cleaning the surface of said substrates incidental to the known methods of vacuum coating, in which the surface of said substrates is cleaned only by the sputtering action of inert gas such as argon, nitrogen and the like.
- inert gas such as argon, nitrogen and the like.
- the present invention succeeded in homogeneously cleaning the surface of said substrates because the smaller sputtering yield can prevent said concave portions or the central portion of said substrates from being contaminated and the reducing reaction by hydrogen can be accelerated by glow discharge. In this case, a still more effective cleaning of said substrates can be attained by simultaneously heating said substrates.
- the sputtering action is too weak when only hydrogen is used as the atmospheric gas. Accordingly, inert gas such as argon, nitrogen and the like may be added to hydrogen. Hydrogen is used at a ratio of 20% by volume or more, preferably at a ratio of 50% by volume or more because the homogeneous adhesive strength of the coating, which is an object of the present invention, cannot be attained if hydrogen is used in an amount below 20% by volume.
- the ion plating method in which the substances to be coated are ionized, is optimum because said hard compounds can be coated on said substrates tightly.
- a process of physical vapor deposition of the present invention is especially effective for said substrates such as gear cutting tools and formed cutters having complex shapes and made of high-speed steel, for example, hobs, pinion cutters and the like.
- the present invention further can provide a process of physical vapor deposition, which is especially effective for the cemented carbide tools or cermet tools, above all for throw away inserts.
- These tools themselves have comparatively simple shapes but it is necessary to rotate said substrates in said physical vapor deposition process in order to attain the homogeneous adhesive strength of the coating to said substrates.
- it is necessary to mount the holder on said substrates which gives complex shapes to an assembly consisting of said substrates and said holder as a whole.
- metals belonging to IVb group, Vb group and VIb group of the Periodic Table be used as materials for vacuum coating on said substrates.
- titanium which has a lower melting point and a higher vapor pressure, can be easily evaporated and its carbide, nitride, carbonitride or compounds consisting of said carbide, nitride or carbonitride of titanium and oxygen form a B-1 type have solid solution and high hardness, chemical stability and welding resistance to iron and steel materials.
- the above mentioned compounds of titanium are industrially the most suitable coating materials.
- An object of the present invention is to give the coating a homogeneous and high adhesive strength regardless of the kind employed. Accordingly, titanium carbide is described as the typical example.
- the ion plating apparatus shown in FIG. 1 was provided with a rotary axis 1 having a holder 3 provided with four tips 2 mounted on said holder 3.
- Said tips were made of high-speed steel SKH4A (Japanese Industrial Standard) having a hardness of H R C 64.5.
- a vacuum chamber 4 was evacuated through a pipe 5 by means of evacuated apparatus 6 until the pressure of 7 ⁇ 10 -3 Pa.
- Said rotary axis 1 was driven by a rotational mechanism 7, said tips 2 being heated to about 400° C. by means of a heater 9 supplied electricity from a power supply 8, and the gas used for sputter cleaning being introduced into said chamber 4 through a pipe for introducing gas used for sputter cleaning 10 until the pressure of 15 Pa.
- Gas used as said atmospheric gas for sputter cleaning includes "hydrogen of 100%" (condition I), “hydrogen of 80%+argon of 20%” (condition II), “hydrogen of 50%+argon of 50%” (condition III), “hydrogen of 30%+argon of 70% (condition IV), “hydrogen of 20%+argon of 80% (condition V), “hydrogen of 10%+argon of 90% (condition VI) and “argon of 100%” (condition VII).
- Sputter cleaning of the surface of said tips was carried out in a glow discharge, which was generated by applying a voltage of -1 kV to said tips by means of a power supply for said substrates 11, for 20 minutes.
- the layer of titanium carbide was formed on the surface of said tips 2 at a thickness of 3 to 3.5 microns.
- Said tips vacuum coated under the above described conditions of I to VII were tested on indentations.
- the tips for the indentation test shown in FIG. 4 were pressed to give indentations at 9 positions of A to I shown in FIG. 5 at a load of 90 kg by means of a Rockwell hardness tester. Whether or not the layer of titanium carbide is peeled off in the periphery of said indentations was dertermined. The results are shown in Table I. o shows the absence of the layer of titanium carbide peeled off while x shows the presence of the layer of titanium carbide peeled off.
- Said tips 2 were made of cemented carbide P30 (72% WC-8% TiC-11% TaC-9% Co) or cermet (40% TiC-15% TiN-10% TaN-10% Mo 2 C-10% WC-10% Co-5% Ni).
- the heating temperature of about 600° C., the pressure of an atmospheric gas used for sputter cleaning of 20 Pa and the compositions of said atmospheric gas used for sputter cleaning of the conditions of I to VII alike in Example 1 were selected.
- Sputter cleaning of the surface of said tips 2 was carried out by glow discharge, which was generated by applying a voltage of -1.5 kV to said substrates 2, for 20 minutes.
- a shutter 19 was opened after the gaseous mixture consisting of acetylene, nitrogen and oxygen at a ratio of 3:6:1 was introduced into said vacuum chamber 4 through a reaction gas pipe 18 until the pressure of 4 ⁇ 10 -2 Pa and titanium oxycarbonitride, that is to say Ti(C 0 .28 N 0 .54 O 0 .18), was deposited on the surface of said tips 2 by the reaction of acetylene, nitrogen and oxygen upon titanium through 90 minutes. As a result the layer of titanium oxycarbonitride was formed on the surface of said tips 2 at a thickness of 4.8 to 5.3 ⁇ m.
- Table 2 shows the results for tips made of cemented carbide while Table 3 shows the results for tips made of cermet.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- ing And Chemical Polishing (AREA)
Abstract
Description
TABLE 1 ______________________________________ Con- Composition of di- gaseous mixtures Positions of test tion Hydrogen Argon A B C D E F G H I ______________________________________ I 100 0 o o o o o o o o o II 80 20 o o o o o o o o o III 50 50 o o x o o o x o o IV 30 70 o o x o o x x x o V 20 80 o o x o o x x x x VI 10 90 o x x x o x x x x VII 0 100 o x x x x x x x x ______________________________________
TABLE 2 ______________________________________ Con- Compostion of di- gaseous mixture Positions of test tion Hydrogen Argon A B C D E F G H I ______________________________________ I 100 0 o o o o o o o o o II 80 20 o o o o o o o o o III 50 50 o o o o o o o o o IV 30 70 o o x o o o x o o V 20 80 o o x o o x x x o VI 10 90 o o x o o x x x x VII 0 100 o o x o o x x x x ______________________________________
TABLE 3 ______________________________________ Con- Composition of di- gaseous mixture Positions of test tion Hydrogen Argon A B C D E F G H I ______________________________________ I 100 0 o o o o o o o o o II 80 20 o o x o o o x o o III 50 50 o o x o o o x o o IV 30 70 o o x o o o x x o V 20 80 o o x o o x x x o VI 10 90 o x x x x x x x x VII 10 100 o x x x x x x x x ______________________________________
Claims (13)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP55-156584 | 1980-11-06 | ||
JP55156584A JPS5779169A (en) | 1980-11-06 | 1980-11-06 | Physical vapor deposition method |
Publications (1)
Publication Number | Publication Date |
---|---|
US4507189A true US4507189A (en) | 1985-03-26 |
Family
ID=15630952
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US06/316,906 Expired - Lifetime US4507189A (en) | 1980-11-06 | 1981-10-30 | Process of physical vapor deposition |
Country Status (5)
Country | Link |
---|---|
US (1) | US4507189A (en) |
JP (1) | JPS5779169A (en) |
DE (1) | DE3144192C2 (en) |
FR (1) | FR2493348B1 (en) |
GB (1) | GB2086943B (en) |
Cited By (29)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4773928A (en) * | 1987-08-03 | 1988-09-27 | Gte Products Corporation | Plasma spray powders and process for producing same |
US4804589A (en) * | 1985-09-26 | 1989-02-14 | Ngk Insulators, Ltd. | Silicon carbide sintered members |
WO1990013422A1 (en) * | 1989-05-05 | 1990-11-15 | Kennametal Inc. | High hardness/high compressive stress multilayer coated tool |
US4990233A (en) * | 1985-06-14 | 1991-02-05 | Permian Research Corporation | Method for retarding mineral buildup in downhole pumps |
DE3936550C1 (en) * | 1989-11-03 | 1991-04-18 | Arthur Klink Gmbh, 7530 Pforzheim, De | Substrate coating for wear resistance - with titanium nitride in vacuum chamber contg. titanium evaporator and heater with rotary substrate holder |
WO1991014017A1 (en) * | 1990-03-09 | 1991-09-19 | Kennametal Inc. | Physical vapor deposition of titanium nitride on a nonconductive substrate |
US5116694A (en) * | 1985-01-21 | 1992-05-26 | Sumitomo Electric Industries, Ltd. | Coated cemented carbides |
US5264297A (en) * | 1990-03-09 | 1993-11-23 | Kennametal Inc. | Physical vapor deposition of titanium nitride on a nonconductive substrate |
WO1994004716A1 (en) * | 1992-08-14 | 1994-03-03 | Hughes Aircraft Company | Surface preparation and deposition method for titanium nitride onto carbonaceous materials |
US5356474A (en) * | 1992-11-27 | 1994-10-18 | General Electric Company | Apparatus and method for making aligned Hi-Tc tape superconductors |
DE4437269C1 (en) * | 1994-10-18 | 1996-02-22 | Balzers Hochvakuum | Cleaning workpiece surfaces |
US5580653A (en) * | 1994-05-13 | 1996-12-03 | Kabushiki Kaisha Kobe Seiko Sho | Hard coating having excellent wear resistance properties, and hard coating coated member |
US5853873A (en) * | 1994-10-27 | 1998-12-29 | Sumitomo Electric Industries, Ltd | Hard composite material for tools |
US5855950A (en) * | 1996-12-30 | 1999-01-05 | Implant Sciences Corporation | Method for growing an alumina surface on orthopaedic implant components |
US5885665A (en) * | 1997-05-09 | 1999-03-23 | The United States Of America As Represented By The United States Department Of Energy | VO2 precipitates for self-protected optical surfaces |
US5922478A (en) * | 1997-04-30 | 1999-07-13 | Masco Corporation | Article having a decorative and protective coating |
WO1999057071A1 (en) * | 1998-05-05 | 1999-11-11 | Corning Incorporated | Material and method for coating glass forming equipment |
US5985468A (en) * | 1997-04-30 | 1999-11-16 | Masco Corporation | Article having a multilayer protective and decorative coating |
US6004684A (en) * | 1997-04-30 | 1999-12-21 | Masco Corporation | Article having a protective and decorative multilayer coating |
US6010750A (en) * | 1997-05-08 | 2000-01-04 | Georgia Tech Research Corporation | Method and apparatus for lithiating alloys |
US6190514B1 (en) | 1997-12-30 | 2001-02-20 | Premark Rwp Holdings, Inc. | Method for high scan sputter coating to produce coated, abrasion resistant press plates with reduced built-in thermal stress |
US6210136B1 (en) * | 1995-10-18 | 2001-04-03 | Matsushita Electric Industrial Co., Ltd. | Scroll compressor and method for manufacturing an oldham ring therefor |
US6338879B1 (en) * | 1998-12-09 | 2002-01-15 | Nachi-Fujikoshi Corp. | Solid lubricant film for coated cutting tool and method for manufacturing same |
US6656329B1 (en) | 1996-08-28 | 2003-12-02 | Premark Rwp Holdings, Inc. | Coated pressing surfaces for abrasion resistant laminate and making laminates therefrom |
US6706448B1 (en) | 1999-08-30 | 2004-03-16 | Georgia Tech Research Corp. | Method and apparatus for lithiating alloys |
US6740167B1 (en) * | 1998-01-29 | 2004-05-25 | Siced Electronics Development Gmbh & Co., Kg | Device for mounting a substrate and method for producing an insert for a susceptor |
US8440328B2 (en) | 2011-03-18 | 2013-05-14 | Kennametal Inc. | Coating for improved wear resistance |
US20130172974A1 (en) * | 2001-11-30 | 2013-07-04 | Advanced Cardiovascular Systems, Inc. | Modified surface for an implantable device and a method of producing the same |
US10718047B2 (en) | 2016-02-09 | 2020-07-21 | Wilsonart Llc | Method for coating stainless steel press plates and coated press plates produced thereby |
Families Citing this family (21)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SE453265B (en) * | 1983-02-14 | 1988-01-25 | Vni Instrument Inst | CUTTING TOOLS WITH RESISTABLE COATING AND PROCEDURES FOR PRODUCING THIS |
JPS60234965A (en) * | 1984-05-04 | 1985-11-21 | Diesel Kiki Co Ltd | Manufacture of thin film |
JPS61183458A (en) * | 1985-02-08 | 1986-08-16 | Citizen Watch Co Ltd | Black ion-plated film |
DE3509572C1 (en) * | 1985-03-16 | 1986-07-10 | Feldmühle AG, 4000 Düsseldorf | Sliding element coated with ceramic material components and its use |
FR2603905A1 (en) * | 1986-09-12 | 1988-03-18 | Elf France | METHOD FOR PROTECTING METAL SURFACES FROM VANADOSODIC CORROSION |
JPH0745707B2 (en) * | 1986-11-25 | 1995-05-17 | 三菱マテリアル株式会社 | Surface-coated titanium carbonitride-based cermet for high-speed cutting |
DK619887A (en) * | 1986-12-01 | 1988-06-02 | Torgau Flachglas | HARDWARE COMPOSITION LAYER ON SILICATIVE SUBSTRATES AND PROCEDURE FOR THEIR PREPARATION |
US5169508A (en) * | 1988-03-04 | 1992-12-08 | Sharp Kabushiki Kaisha | Graphite electrode |
JPH0722018B2 (en) * | 1988-03-04 | 1995-03-08 | シャープ株式会社 | Method of manufacturing graphite electrode |
US5436071A (en) * | 1990-01-31 | 1995-07-25 | Mitsubishi Materials Corporation | Cermet cutting tool and process for producing the same |
US5039570A (en) * | 1990-04-12 | 1991-08-13 | Planar Circuit Technologies, Inc. | Resistive laminate for printed circuit boards, method and apparatus for forming the same |
DE4034842A1 (en) * | 1990-11-02 | 1992-05-07 | Thyssen Edelstahlwerke Ag | METHOD FOR PLASMA MECHANICAL CLEANING FOR A SUBSEQUENT PVD OR PECVD COATING |
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BE1009839A3 (en) * | 1995-12-20 | 1997-10-07 | Cockerill Rech & Dev | Method and device for cleaning substrate metal. |
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JP5250321B2 (en) * | 2008-07-04 | 2013-07-31 | 昭和電工株式会社 | Method for producing seed crystal for silicon carbide single crystal growth and method for producing silicon carbide single crystal |
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-
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- 1981-11-06 FR FR8120807A patent/FR2493348B1/en not_active Expired
- 1981-11-06 DE DE3144192A patent/DE3144192C2/en not_active Expired
- 1981-11-06 GB GB8133589A patent/GB2086943B/en not_active Expired
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Cited By (39)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5116694A (en) * | 1985-01-21 | 1992-05-26 | Sumitomo Electric Industries, Ltd. | Coated cemented carbides |
US4990233A (en) * | 1985-06-14 | 1991-02-05 | Permian Research Corporation | Method for retarding mineral buildup in downhole pumps |
US4804589A (en) * | 1985-09-26 | 1989-02-14 | Ngk Insulators, Ltd. | Silicon carbide sintered members |
US4773928A (en) * | 1987-08-03 | 1988-09-27 | Gte Products Corporation | Plasma spray powders and process for producing same |
WO1990013422A1 (en) * | 1989-05-05 | 1990-11-15 | Kennametal Inc. | High hardness/high compressive stress multilayer coated tool |
US5075181A (en) * | 1989-05-05 | 1991-12-24 | Kennametal Inc. | High hardness/high compressive stress multilayer coated tool |
DE3936550C1 (en) * | 1989-11-03 | 1991-04-18 | Arthur Klink Gmbh, 7530 Pforzheim, De | Substrate coating for wear resistance - with titanium nitride in vacuum chamber contg. titanium evaporator and heater with rotary substrate holder |
US5858181A (en) * | 1990-03-09 | 1999-01-12 | Kennametal Inc. | Physical vapor deposition of titanium nitride on a nonconductive substrate |
WO1991014017A1 (en) * | 1990-03-09 | 1991-09-19 | Kennametal Inc. | Physical vapor deposition of titanium nitride on a nonconductive substrate |
US5264297A (en) * | 1990-03-09 | 1993-11-23 | Kennametal Inc. | Physical vapor deposition of titanium nitride on a nonconductive substrate |
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Also Published As
Publication number | Publication date |
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DE3144192A1 (en) | 1982-07-29 |
GB2086943A (en) | 1982-05-19 |
JPS5779169A (en) | 1982-05-18 |
FR2493348B1 (en) | 1985-10-04 |
GB2086943B (en) | 1985-09-25 |
DE3144192C2 (en) | 1983-12-29 |
FR2493348A1 (en) | 1982-05-07 |
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